CN106241816A - A kind of preparation method of silica dioxide delustring agent - Google Patents
A kind of preparation method of silica dioxide delustring agent Download PDFInfo
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- CN106241816A CN106241816A CN201610571495.2A CN201610571495A CN106241816A CN 106241816 A CN106241816 A CN 106241816A CN 201610571495 A CN201610571495 A CN 201610571495A CN 106241816 A CN106241816 A CN 106241816A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
Abstract
The present invention provides the preparation method of the silica dioxide delustring agent that a kind of big pore volume, pore-size distribution concentrate, comprise the steps: step 1, in pure water, add one or more in ethylene glycol, n-butyl alcohol and ethanol, by adding sodium hydroxide after steam intensification 50～60 DEG C, obtain bottom water, waterglass and dilute sulfuric acid is added in the bottom water being stirred continuously, controlling pH value of reaction system and keep constant, the response time is 30～90min；After reaction terminates, continuously adding dilute sulfuric acid to pH value of reaction system is 3～4, obtains reaction paste；Step 2, to control reaction paste pH value be 7.5～10.5, is warming up to 80～95 DEG C of reactions 1～3h, then to be acidified to pH value be 3～4.The beneficial effects of the present invention is: keep constant by adding sodium hydroxide solution and dilute sulfuric acid in bottom water simultaneously to control pH value of reaction system, obtain large aperture and even aperture distribution silicon dioxide microcellular structure.
Description
Technical field
The present invention relates to delustering agent field, the preparation method of a kind of silica dioxide delustring agent.
Background technology
Big pore volume high efficiency delustering agent silicon dioxide production technology comprises following production stage: (one) waterglass is prepared
(2) preparation of dilute sulfuric acid, (three) soda acid also flows gel synthesis (four) gel is aging and reaming (five) sheet frame washing (five) spray dried
Dry and pulverize.
At present, the big pore volume delustering agent commonly used sol-gel process of silicon dioxide production technology produces, the macropore of production
Hold delustering agent and there is following shortcoming:
1, produce, owing to the volume of the limitation reactor of technique is little at 1-10m with enamel reaction3Volume, produce effect
Rate is low, energy consumption is high, the poor stability of product.
2, plastic mode use first add waterglass be end liquid stir acid adding plastic, reaction mechanism is the sodium oxide solubility of end alkali
From high to low, the pH value of reaction system is also from high to low, and the precursor size of the silicon dioxide of generation is uneven, titanium dioxide
The particle agglomeration of silicon is serious, causes follow-up gel aging and during reaming, and pore volume volume is little, pore-size distribution width, flatting efficiency low and
Bad dispersibility.
Summary of the invention
The technical problem to be solved is: provide the silicon dioxide delustring that a kind of big pore volume, pore-size distribution are concentrated
The preparation method of agent.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is: the preparation method of silica dioxide delustring agent,
Comprise the steps:
Step 1, in pure water, add one or more in ethylene glycol, n-butyl alcohol and ethanol, by steam heat up 50～
Add sodium hydroxide after 60 DEG C, obtain bottom water, in the bottom water being stirred continuously, add waterglass and dilute sulfuric acid, control reaction system pH
Value keeps constant, and the response time is 30～90min；
After reaction terminates, continuously adding dilute sulfuric acid to pH value of reaction system is 3～4, obtains reaction paste；
Step 2, control reaction paste pH value are 7.5～10.5, are warming up to 80～95 DEG C of reactions 1～3h, then are acidified to pH
Value is 3～4.
Further, also include:
Step 3, by step 2 gains washing to filter electrical conductivity of water ＜ 50 μ S/cm, after slurrying, defibrination, spray drying
Pulverized by jet mill, obtain silica dioxide delustring agent.
Further, H in described dilute sulfuric acid2SO4Mass fraction be 5～30%.
Further, SiO in described waterglass2Mass fraction be 5～25%.
Further, in step 2, by adding sodium hydroxide solution, ammonia or ammonium in the reaction paste being stirred continuously
It is 7.5～10.5 that saline solution controls reaction paste pH value.
The beneficial effects of the present invention is: bottom water adds a certain amount of ethylene glycol, n-butyl alcohol, ethanol at a proper temperature
Deng alcohols, plastic reaction (step 1) is to use soda acid and flow direct reaction plastic in bottom water simultaneously, and it is the fiercest to react, and becomes
Core speed is fast, the beneficially generation of crystalline silica nuclei, is conducive to generating the spherical simple particle diameter of size uniformly rule, aging
And reaming reaction (step 2) time, high temperature, subalkaline under the conditions of, small particles dissolve grow into bulky grain, obtain big pore volume,
The microporous structure that pore-size distribution is concentrated.
Detailed description of the invention
By describing the technology contents of the present invention in detail, being realized purpose and effect, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is: add one or more in ethylene glycol, n-butyl alcohol and ethanol in pure water,
Adding sodium hydroxide, the pH value of front bottom water system is reacted in regulation, it is ensured that start pH value in reaction pre-add bottom water system front with reaction
PH value is consistent, and course of reaction pH value of reaction system keeps stable.Dilute sulfuric acid, waterglass also flow addition, use and determine alkali Flow-rate adjustment
The pH value of liquid at the bottom of acid flow-control so that the precursor size of generation silicon dioxide is uniform, the particle dispersion of silicon dioxide
Good；When follow-up aging and reaming is reacted, under the conditions of high temperature is subalkaline, small particles is dissolved and is grown into bulky grain, obtains big
Aperture and even aperture distribution silicon dioxide microcellular structure.
The present invention provides the preparation method of a kind of silica dioxide delustring agent, comprises the steps:
Step 1, in pure water, add one or more in ethylene glycol, n-butyl alcohol and ethanol, by steam heat up 50～
Add sodium hydroxide after 60 DEG C, obtain bottom water, in the bottom water being stirred continuously, add waterglass and dilute sulfuric acid, control reaction system pH
Value keeps constant, and the response time is 30～90min；
After reaction terminates, continuously adding dilute sulfuric acid to pH value of reaction system is 3～4, obtains reaction paste；
Step 2, control reaction paste pH value are 7.5～10.5, are warming up to 80～95 DEG C of reactions 1～3h, then are acidified to pH
Value is 3～4.
Knowable to foregoing description, the beneficial effects of the present invention is: utilize conventional stainless steel cauldron 45-120m3Raw
Become delustering agent silica product, in reactor, add tap water in advance, add the pH of a certain amount of Caustic soda regulation bottom water
Value, controls reaction process temperature, opens stirring, passes through acid, alkali pipeline respectively and flow addition, using and determine alkali Flow-rate adjustment acid flow
Control the pH value of end liquid, it is ensured that pH value at the beginning is consistent with the pH value of pre-add bottom water system before reaction, course of reaction reactant
It is that pH value keeps stable.The precursor size particle dispersion uniform, silicon dioxide generating silicon dioxide is good, follow-up gel
During aging and reaming, pore volume volume is big, pore-size distribution is concentrated, and flatting efficiency is high and good dispersion.During aging and reaming reaction,
Under the conditions of high temperature is subalkaline, small particles is dissolved and is grown into bulky grain, obtains uniform large aperture silicon dioxide microcellular structure.
Adding the alcohols such as a certain amount of ethylene glycol, n-butyl alcohol, ethanol at a proper temperature in bottom water, plastic reaction is to use
Soda acid also flows direct reaction plastic in bottom water, and it is the fiercest to react, and nucleation rate is fast, the beneficially life of crystalline silica nuclei
Become, be conducive to generating the spherical simple particle diameter of size uniformly rule, when aging and reaming reaction, big pore volume, aperture can be obtained
The microporous structure that distribution is concentrated.Utilize big volume reactor 45-120m3, production efficiency is high, energy consumption is low, the stability of product
Good, production technology is simply more beneficial for industrialized production.
Further, also include:
Step 3, by step 2 gains washing to filter electrical conductivity of water ＜ 50 μ S/cm, after slurrying, defibrination, spray drying
Pulverized by jet mill, obtain silica dioxide delustring agent.
Further, H in described dilute sulfuric acid2SO4Mass fraction be 5～30%.
Further, SiO in described waterglass2Mass fraction be 5～25%.
Further, in step 2, by adding sodium hydroxide solution, ammonia or ammonium in the reaction paste being stirred continuously
It is 7.5～10.5 that saline solution controls reaction paste pH value.
To sum up, the present invention provide silica dioxide delustring agent preparation method particularly as follows:
Step 1, preparation SiO2Mass fraction is 5～the waterglass of 25% and H2SO4Mass fraction is dilute sulfur of 5～30%
Acid；
Step 2, in pure water, add one or more in ethylene glycol, n-butyl alcohol and ethanol, by steam heat up 50～
Add sodium hydroxide after 60 DEG C, obtain bottom water, in the bottom water being stirred continuously, add waterglass and dilute sulfuric acid, control reaction system pH
Value keeps constant, and the response time is 30～90min；
After reaction terminates, continuously adding dilute sulfuric acid to pH value of reaction system is 3～4, obtains reaction paste；
Step 3,
In the reaction paste being stirred continuously, add sodium hydroxide solution, ammonia or ammonium salt solution, control reaction paste pH
Value is 7.5～10.5, is warming up to 80～95 DEG C of reactions 1～3h, then to be acidified to pH value be 3～4；
Step 4, by step 3 gains with pure water to filter electrical conductivity of water ＜ 50 μ S/cm, through slurrying, defibrination, spraying
Pulverized by jet mill after drying, obtain silica dioxide delustring agent.
Embodiment 1
Waterglass be formulated as modulus 3.3, SiO2Mass fraction be 15%, dilute sulfuric acid mass fraction is 15%.At 90m3
In reactor, it is initially charged 20m3Pure water, add 20kg ethylene glycol, be passed through steam heat up, be warming up to 55 DEG C, open stirring, add
Entering pH value=8 of 2kg Caustic soda regulation bottom water, the temperature controlling reaction is 55 DEG C, adds the waterglass prepared in reactor
With dilute sulfuric acid flow reaction, the soda acid flow rate ratio reacted by adjustment is controlled pH value=8 of reaction, makes pH value in reaction and the end
The pH value of water keeps consistent, and the response time controlled at 60 minutes, and flows reaction and terminate.Continuously add dilute sulfuric acid and be acidified to pH value
3.5.In reactor, it is initially charged in 10L Caustic soda and 150L30% ammonia the dilute sulfuric acid closing excess, regulates reaction paste pH value 8.5
Alkalescence under, be warming up to aging reaction 2 hours under the high temperature of 90 DEG C, then be acidified to pH value=3. reaction paste with dilute sulfuric acid
Inject filtrating-pressing plate frame, first with the tap water washing after filtration, wash to drainage electrical conductivity ＜ 200 μ S/cm, then with pure water extremely
Filter electrical conductivity of water ＜ 50 μ S/cm, slurrying, defibrination, it is spray-dried, is pulverized by jet mill.
Embodiment 2
Waterglass be formulated as modulus 3.35, SiO2Mass fraction be 18%, dilute sulfuric acid mass fraction is 25%.?
90m3In reactor, it is initially charged 30m3Pure water, add 20kg Polyethylene Glycol, be passed through steam heat up, be warming up to 65 DEG C, unlatching is stirred
Mixing, add 5kg Caustic soda and regulate pH value=8.5 of bottom water, the temperature controlling reaction is 65 DEG C, and in reactor, addition prepares
Waterglass and dilute sulfuric acid also flow reaction, and the soda acid flow rate ratio reacted by adjustment controls pH value=8.5 of reaction, makes reaction
PH value and the pH value of bottom water keep consistent, and the response time controlled at 60 minutes, and flow reaction and terminate.Continuously add dilute sulfuric acid acidifying
To pH value 3.5.In reactor, it is initially charged in 10L Caustic soda and 100L30% ammonia the dilute sulfuric acid closing excess, regulates reaction paste
Under the alkalescence of pH value 8.0, it is warming up to aging reaction 2 hours under the high temperature of 95 DEG C, then is acidified to pH value=3 with dilute sulfuric acid.?
Reaction paste injects filtrating-pressing plate frame, first with the tap water washing after filtration, washs to drainage electrical conductivity ＜ 200 μ S/cm, then with pure
Water washing, to filter electrical conductivity of water ＜ 50 μ S/cm, slurrying, defibrination, is spray-dried, is pulverized by jet mill.
Embodiment 3
Waterglass be formulated as modulus 3.45, SiO2Mass fraction be 22%, dilute sulfuric acid mass fraction is 30%.?
90m3In reactor, it is initially charged 35m3Pure water, add 20kg n-butyl alcohol, be passed through steam heat up, be warming up to 50 DEG C, open stirring,
Adding pH value=8.5 of 5kg Caustic soda regulation bottom water, the temperature controlling reaction is 50 DEG C, adds the water prepared in reactor
Glass and dilute sulfuric acid also flow reaction, and the soda acid flow rate ratio reacted by adjustment controls pH value=8.5 of reaction, makes reaction PH
Value is consistent with the holding of the pH value of bottom water, and the response time controlled at 45 minutes, and flowed reaction and terminate.Continuously add dilute sulfuric acid to be acidified to
PH value 3.5.In reactor, it is initially charged in 10L Caustic soda and 80L30% ammonia the dilute sulfuric acid closing excess, regulates reaction paste pH value
Under the alkalescence of 7.5, it is warming up to aging reaction 2 hours under the high temperature of 95 DEG C, then is acidified to pH value=3 with dilute sulfuric acid.Reaction
Slurry injects filtrating-pressing plate frame, and first with the tap water washing after filtration, washing is to drainage electrical conductivity ＜ 200 μ S/cm, then washes with pure water
Wash to filter electrical conductivity of water ＜ 50 μ S/cm, slurrying, defibrination, be spray-dried, pulverized by jet mill.
Embodiment 4
Waterglass be formulated as modulus 3.3, SiO2Mass fraction be 10%, dilute sulfuric acid mass fraction is 15%.At 90m3
In reactor, it is initially charged 15m3Pure water, add 20kg ethylene glycol, be passed through steam heat up, be warming up to 50 DEG C, open stirring, add
Entering pH value=10.5 of 5kg Caustic soda regulation bottom water, the temperature controlling reaction is 50 DEG C, adds the water glass prepared in reactor
Glass and dilute sulfuric acid also flow reaction, and the soda acid flow rate ratio reacted by adjustment controls pH value=10.5 of reaction, makes reaction pH
Value is consistent with the holding of the pH value of bottom water, and the response time controlled at 90 minutes, and flowed reaction and terminate.Continuously add dilute sulfuric acid to be acidified to
PH value 3.5.In reactor, it is initially charged in 10L Caustic soda and 120L30% ammonia the dilute sulfuric acid closing excess, regulates reaction paste pH
Under the alkalescence of value 8.0, it is warming up to aging reaction 2 hours under the high temperature of 90 DEG C, then is acidified to pH value=3 with dilute sulfuric acid.Anti-
Answering slurry to inject filtrating-pressing plate frame, first with the tap water washing after filtration, washing is to drainage electrical conductivity ＜ 200 μ S/cm, then uses pure water
Washing, to filter electrical conductivity of water ＜ 50 μ S/cm, slurrying, defibrination, is spray-dried, is pulverized by jet mill.
Every testing result of the silica dioxide delustring agent of embodiment 1～4 gained is shown in Table 1.
Table 1
| Title | BET(m2/g) | DBP(ml/g) | Pore volume (cm3/g) | Aperture (nm) |
| Embodiment 1 | 325 | 2.60 | 1.95 | 21 |
| Embodiment 2 | 350 | 2.65 | 1.98 | 22 |
| Embodiment 3 | 305 | 2.68 | 2.00 | 22 |
| Embodiment 4 | 315 | 2.58 | 1.92 | 20 |
Embodiment 5
The concrete preparation process of inventive silica delustering agent is as follows:
Step 1, waterglass are prepared
The solid water glass modulus of the low ferrum of selected high-quality controls 2.5-3.6, adds at reverse osmosis membrane in putting into cylinder rotary spherical digester
The water (hereinafter referred to as pure water) of reason, is passed through the rotary spherical digester through accurate filter, is forced into 0.6MPA, pressurize 2 hours.Concentrated sodium silicate
Add the water of reverse osmosis membrane processing, be configured to SiO2Mass fraction is the solution of 5-25%, stores standby.
Step 2, the preparation of dilute sulfuric acid
Concentrated sulphuric acid is configured to mass fraction H by graphite nitration mixture condenser2SO4Be 5～30% dilute sulfuric acid collect standby.
Step 3, soda acid also flow gel synthesis
At 90m3In reactor, it is initially charged a certain amount of pure water, adds the alcohol such as a certain amount of ethylene glycol, n-butyl alcohol, ethanol
Class, is passed through steam and heats up, and adds the pH value of a certain amount of Caustic soda regulation bottom water, controls the temperature of reaction, open stirring, toward reactor
Waterglass that interior addition prepares and dilute sulfuric acid also flow reaction, and the soda acid flow rate ratio reacted by adjustment controls the pH of reaction
Value, makes the holding of pH value in reaction and the pH value of bottom water consistent, and the response time controlled at 30-90 minute, and flows reaction and terminate.Continue to add
Enter dilute sulfuric acid and be acidified to pH value 3-4.
Step 4, gel be aging and reaming
The dilute sulfuric acid closing excess in the ammonium salt species such as Caustic soda, ammonia, ammonium hydrogen carbonate, reaction paste pH is added in reactor
Under the alkalescence of value 7.5-10.5, it is warming up to aging reaction 1-3 hour under the high temperature of 80-95 DEG C, then is acidified to pH with dilute sulfuric acid
Value=3-4.
Step 5, sheet frame material feeding washing
First with the tap water washing after filtration, then with pure water to filtering electrical conductivity of water ＜ 50 μ S/cm, slurrying, defibrination,
It is spray-dried, is pulverized by jet mill.
In sum, the having the beneficial effects that of preparation method of the silica dioxide delustring agent that the present invention provides: suitable
At a temperature of bottom water adds the alcohols such as a certain amount of ethylene glycol, n-butyl alcohol, ethanol, plastic reaction (step 1) is to use soda acid simultaneously
And flow direct reaction plastic in bottom water, it is the fiercest to react, and nucleation rate is fast, and beneficially the generation of crystalline silica nuclei, has
It is beneficial to generate the spherical simple particle diameter of size uniformly rule, when aging and reaming reaction (step 2), big pore volume, hole can be obtained
The microporous structure that footpath distribution is concentrated.
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every utilize this
The equivalents that bright description is made, or directly or indirectly it is used in relevant technical field, the most in like manner it is included in this
In bright scope of patent protection.
Claims (5)
1. the preparation method of a silica dioxide delustring agent, it is characterised in that comprise the steps:
Step 1, in pure water, add one or more in ethylene glycol, n-butyl alcohol and ethanol, heated up 50～60 DEG C by steam
Rear addition sodium hydroxide, obtains bottom water, adds waterglass and dilute sulfuric acid in the bottom water being stirred continuously, and controls pH value of reaction system and protects
Holding constant, the response time is 30～90min；
After reaction terminates, continuously adding dilute sulfuric acid to pH value of reaction system is 3～4, obtains reaction paste；
Step 2, to control reaction paste pH value be 7.5～10.5, is warming up to 80～95 DEG C of reactions 1～3h, then to be acidified to pH value be 3
～4.
The preparation method of silica dioxide delustring agent the most according to claim 1, it is characterised in that also include:
Step 3, by step 2 gains washing to filter electrical conductivity of water ＜ 50 μ S/cm, pass through after slurrying, defibrination, spray drying
Jet mill is pulverized, and obtains silica dioxide delustring agent.
The preparation method of silica dioxide delustring agent the most according to claim 1, it is characterised in that H in described dilute sulfuric acid2SO4
Mass fraction be 5～30%.
The preparation method of silica dioxide delustring agent the most according to claim 1, it is characterised in that SiO in described waterglass2
Mass fraction be 5～25%.
The preparation method of silica dioxide delustring agent the most according to claim 1, it is characterised in that in step 2, by not
Add sodium hydroxide solution, ammonia or ammonium salt solution in the reaction paste of disconnected stirring controlling reaction paste pH value is 7.5～10.5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107245904A (en) * | 2017-06-06 | 2017-10-13 | 福建远翔新材料股份有限公司 | A kind of production method of high-performance ink-jet paper silica ink absorbent |
| CN110607197A (en) * | 2019-08-23 | 2019-12-24 | 广州凌玮科技股份有限公司 | Antirust lubricating oil |
| CN111825098A (en) * | 2020-07-15 | 2020-10-27 | 确成硅化学股份有限公司 | High-dispersion large-pore-volume narrow-pore-diameter-distribution hydrated silicon dioxide and preparation method thereof |
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| CN105712361A (en) * | 2016-03-24 | 2016-06-29 | 通化双龙化工股份有限公司 | Production method of food additive white carbon black |
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| US3959174A (en) * | 1971-08-24 | 1976-05-25 | W. R. Grace & Co. | Method of selectively producing high pore volume silica gel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109403138B (en) * | 2017-06-06 | 2021-02-02 | 福建远翔新材料股份有限公司 | Production method of high-dispersion silicon dioxide ink absorber for color spray paper |
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| CN111825098A (en) * | 2020-07-15 | 2020-10-27 | 确成硅化学股份有限公司 | High-dispersion large-pore-volume narrow-pore-diameter-distribution hydrated silicon dioxide and preparation method thereof |
| CN111825098B (en) * | 2020-07-15 | 2023-10-27 | 确成硅化学股份有限公司 | High-dispersion large-pore-volume pore-diameter narrow-distribution hydrated silicon dioxide and preparation method thereof |
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| CN106241816B (en) | 2018-04-17 |
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